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1.
多功能柱净化-高效液相色谱法检测谷物中的玉米赤霉烯酮 总被引:7,自引:0,他引:7
建立了玉米和小麦中玉米赤霉烯酮(ZEN)的多功能柱净化-高效液相色谱检测方法。样品经乙腈-水混合溶剂(V(乙腈):V(水)=84:16)提取,通过多功能净化柱(MFC)进行一次性净化,以Symmetry^R C18柱为分离柱,甲醇-水(V(甲醇):V(水)=68:32)为流动相进行高效液相色谱分离和检测。玉米赤霉烯酮的质量浓度在0.01~4.0μg/mL范围内呈良好线性,相关系数为0.9996。检出限为0.04μg/g,在0、04—5.0mg/kg添加范围内的回收率为87.5%~98.6%,相对标准偏差为1.5%~8.3%。 相似文献
2.
Aldo Laganà Angelo Faberi Giovanna Fago Aldo Marino Elisabetta Pastorini Roberto Samperi 《International journal of environmental analytical chemistry》2013,93(13):1009-1016
The metabolic fate of the estrogenic mycotoxin zearalenone in rainbow trout is presently unknown. In this study, the tissue concentration of zearalenone and its principal metabolites (α-zearalenol and β-zearalenol) was determined. A known amount of zearalenone was administered as a single bolus to ten fish, and the biological tissue concentration was determined at various times following administration. The analytes were extracted from liver and muscular tissue using an on-line matrix solid-phase dispersion–solid-phase extraction sample preparation protocol, and their concentration determined by HPLC–Turboionspray–tandem mass spectrometry. The results showed that zearalenone is mainly metabolized into α-zearalenol in both liver and muscular tissues. The maximum concentrations of each analyte found in liver were 76.1, 211.2 and 63.7?ng/g respectively for zearalenone, α-zearalenol and β-zearalenol, while in muscular tissue they were 10.7, 8.2 and 6.5?ng/g. These values were reached after 2?h in liver tissue and 12?h in muscular tissue. Moreover the data obtained showed that the elimination rate in liver is quite fast since 48?h after the exposure less than 7% of the maximum concentration found is still present. In muscular tissue, however, about one-third of the maximum concentration found is still present after 48?h. 相似文献
3.
Mycotoxins: Simultaneous Detection of Zearalenone and Citrinin by Voltammetry on Edge Plane Pyrolytic Graphite Electrode 下载免费PDF全文
Mycotoxins are highly toxic compounds often found in the food. It is of paramount importance to have analytical technique for point‐of‐care on‐spot detection for authorised personnel to immediately take the action required. Electrochemistry offers the portability for miniaturized sensor of mycotoxins. Here we show that edge‐plane pyrolytic electrode offers excellent selectivity and sensitivity towards simultaneous detection of zearalenone and citrinin. This will have a great impact for point‐of‐care mycotoxin detection. 相似文献
4.
The mycotoxin zearalenone (ZEA) prompts reproductive toxicity due to its strong estrogenic effects. In this work, an electrochemical sensor for determination of ZEA was developed by electropolymerization of a molecularly imprinted poly (o‐phenylenediamine) (PPD) film on screen‐printed gold electrode (SPGE) surface. The sensor was examined by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) using K3[Fe(CN)6]/K4[Fe(CN)6] as redox probe. The molecularly imprinted polymer (MIP) sensor showed a wide determination range from 2.50 to 200.00 ngmL?1 for ZEA. The Limit of detection (LOD) was calculated to be 0.20 ngmL?1, based on the signal to noise (S/N) ratio equal to 3.0. The sensor displayed good repeatability, with RSD values≤4.6 %, and maintained 93.2 % of its initial response after storage for 10 days in air at room temperature. The developed method was successfully applied for the determination of ZEA in corn flakes with mean recoveries ranged from 96.2 % to 103.8 % and RSDs within the interval of 2.1 % to 3.8 %. 相似文献
5.
David Siegel Karsten Andrae Matthias Proske Cindy Kochan Matthias Koch Marcus Weber Irene Nehls 《Journal of chromatography. A》2010,1217(15):2206-2215
A novel, cost-efficient method for the analytical extraction of the Fusarium mycotoxin zearalenone (ZON) from edible oils by dynamic covalent hydrazine chemistry (DCHC) was developed and validated for its application with high performance liquid chromatography-fluorescence detection (HPLC-FLD). ZON is extracted from the edible oil by hydrazone formation on a polymer resin functionalised with hydrazine groups and subsequently released by hydrolysis. Specifity and precision of this approach are superior to liquid partitioning or gel permeation chromatography (GPC). DCHC also extracts zearalanone (ZAN) but not α-/β-zearalenol or -zearalanol. The hydrodynamic properties of ZON, which were estimated using molecular simulation data, indicate that the compound is unaffected by nanofiltration through the resin pores and thus selectively extracted. The method's levels of detection and quantification are 10 and 30 μg/kg, using 0.2 g of sample. Linearity is given in the range of 10–20,000 μg/kg, the average recovery being 89%. Bias and relative standard deviations do not exceed 7%. In a sample survey of 44 commercial edible oils based on various agricultural commodities (maize, olives, nuts, seeds, etc.) ZON was detected in four maize oil samples, the average content in the positive samples being 99 μg/kg. The HPLC-FLD results were confirmed by HPLC–tandem mass spectrometry and compared to those obtained by a liquid partitioning based sample preparation procedure. 相似文献
6.
7.
Blokland MH Sterk SS Stephany RW Launay FM Kennedy DG van Ginkel LA 《Analytical and bioanalytical chemistry》2006,384(5):1221-1227
An EU project, FAIR5-CT-1997-3443, has been undertaken to distinguish illegal use of zeranol from consumption of food contaminated
with Fusarium spp. toxin. One of the tasks was development of screening and confirmatory methods of analysis. This paper describes a new method
based on two-step clean-up and GC–MS analysis. The first clean-up step is matrix-dependant; the second is applicable to both
urine and meat. The MS is operated in negative chemical ionisation mode. The method is quantitative for zeranol and taleranol,
α- and β-zearalenol, and zearalenone and qualitative for zearalanone. Validation was performed according to the latest EU
performance criteria (Commission Decision 2002/657). For analysis of urine and for the method (μg L−1) were 0.06–0.11 for zeranol, 0.07–0.12 for taleranol, 0.07–0.11 for α-zearalenol, 0.21–0.36 for β-zearalenol, 0.35–0.60 for
zearalenone, and 0.19–0.33 zearalanone. Within-laboratory reproducibility was 16.2, 11.2, 31.9, 30.1, 26.6, and 54.2% for
zeranol, taleranol, α-zearalenol, β-zearalenol, zearalenone, and zearalanone, respectively. It was found that all the compounds
are stable in urine at −20°C for at least a year. Part of the validation program was organisation of a small proficiency study
(ringtest) and a correlation study with an LC–MS–MS method developed by the Veterinary Science Division (VSD; Belfast, UK-NI).
This study showed there was good correlation between results from both laboratories. The method can be used for quantitative
analysis discriminating illegal use of zeranol from consumption of zearalenone-contaminated food. 相似文献
8.
Josephs RD Krska R MacDonald S Wilson P Pettersson H 《Analytical and bioanalytical chemistry》2004,378(5):1182-1189
Several previous interlaboratory studies in the field of mycotoxin analysis have revealed considerable problems, apparent as high between-laboratory standard deviations, or rather non-comparable and non-traceable results. A major reason is lack of proper calibrants for external calibration. Public awareness of substances that mimic or interfere with the activity of natural hormones (endocrine disrupters) has led to increased interest in mycotoxins with estrogenic potential, e.g. zearalenone (ZON). During a large-scale standard measurement and testing (SMT) project of the European Commission (EC) dealing with the preparation and certification of reference materials for determination of the mycotoxin ZON in maize, a ZON calibrant in acetonitrile was prepared and intensively checked for purity, homogeneity, and stability. Preparation of the material, study of its homogeneity and stability, and characterisation of the calibrant on the basis of its preparation, with discussion of the results obtained, are described in this paper. The certified value of 9.95 µg mL–1 for ZON in acetonitrile and its corresponding expanded uncertainty of ±0.30 µg mL–1 were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM). 相似文献
9.
《Electrophoresis》2018,39(16):2125-2130
A double‐label immunochromatographic based assay (DL‐ICA) was developed to monitor zearalenone (ZEN) levels in cereals, based on Eu3+ nanoparticles (EuNP). The DL‐ICA exhibited excellent sensitivity, reliability and selectivity in real samples. It showed low limits of detection (0.21–0.25 μg/kg) and broad analytical ranges (up to 120 μg/kg). The total analytical time, including sample preparation and DL‐ICA execution, was reduced by 15 min compared with HPLC. The recovery rates ranged from 95.0–118.4%, with relative standard deviations (RSD) <11.6%. Inter‐ and intra‐day validations were assessed, recovery rates of 89.3–106.9% and RSD of 2.3–9.7% were obtained, suggesting considerable stability and reliability for the assay. An excellent correlation was observed between DL‐ICA and a reference HPLC method (R2 = 0.9899). Compared to current immunoassays, the current DL‐ICA is inexpensive, highly sensitive, and rapid. Therefore, DL‐ICA constitutes a novel tool for monitoring mycotoxins in food and feed to ensure safety. 相似文献
10.
A new method for the fluorometric determination of zearalenone (ZEN) based on its reaction with βNADH in the presence of the enzyme 3α-hydroxysteroid dehydrogenase (3α-HSD) is described. The procedure is based on the change in fluorescence intensity that takes place during the enzymatic reaction (excitation at 340 nm and emission at 454 nm). The optimum reaction conditions and the analytical characteristics were studied; linear response range (1-10 mg l−1) and reproducibility (8 mg l−1, 2.7%, n=7). Moreover, a mathematical model explaining the analytical signal is proposed. The method has been applied to zearalenone determination in a spiked corn sample. 相似文献